CN110364420B - Epitaxial growth method for improving quality of nonpolar GaN material by inserting InGaN/GaN superlattice structure - Google Patents
Epitaxial growth method for improving quality of nonpolar GaN material by inserting InGaN/GaN superlattice structure Download PDFInfo
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Abstract
The invention provides a method for improving the epitaxial quality of a nonpolar GaN material by inserting an InGaN/GaN superlattice structure, which is an epitaxial growth method for reducing the dislocation density of the nonpolar GaN material and improving the surface appearance of an epitaxial wafer so as to improve the material quality. By utilizing a Metal Organic Chemical Vapor Deposition (MOCVD) technology, an epitaxial structure sequentially comprises an r-plane sapphire substrate and a low-temperature GaN nucleating layer from bottom to top; a high-temperature three-dimensional GaN layer grown under the growth conditions of high pressure and high V/III ratio (molar flow ratio of V-group source to III-group source); a high-temperature two-dimensional GaN layer grown under the growth conditions of low pressure and low V/III ratio for the first time; an InGaN/GaN superlattice structure insertion layer; and growing a high-temperature two-dimensional GaN layer under the conditions of low pressure and low V/III ratio for the second time. The invention is characterized in that an InGaN/GaN superlattice structure insertion layer is inserted into the two-dimensional GaN layer, which can relieve stress and prevent transmission of threading dislocation generated by mismatch of a part of the sapphire substrate and epitaxially grown GaN material. The invention can reduce the dislocation density of the nonpolar GaN material, improve the surface appearance and improve the quality of the epitaxial wafer.
Description
The technical field is as follows:
the invention belongs to the technical field of GaN material epitaxy, and relates to a technology for improving the quality of a nonpolar GaN material and reducing dislocation.
Background art:
gallium nitride (GaN) is a direct band gap material, has the characteristics of forbidden bandwidth, stable chemical property and high temperature resistance, and is widely applied to light emittersDevices such as devices, photodetectors, solar cells, and the like. At present, commercially produced GaN devices are all prepared on a c-plane sapphire substrate, the GaN devices grow along a polar axis c axis, materials have a polarization effect, and a strong polarization electric field can appear in an active region of the devices, so that electron hole pairs are separated, a quantum confinement Stark effect is generated, and the luminous efficiency is reduced. To avoid polarization effects, nonpolar GaN materials and devices can be grown, which means that the growth direction is perpendicular to the polar axis [0001 ]]In a direction, e.g. along [11 ]20]The directional growth, the non-polar GaN film can eliminate the polarization electric field, which is beneficial to improving the quantum efficiency of the device. But due to the edge [11 ]20]The directionally grown a-plane nonpolar GaN material is positioned at the c-axis [0001 ] in the growth plane]And m axis [1 ]100]Different mismatch can be brought by different lattice constants along the direction, the mismatch along the c axis is 1.2%, and the mismatch along the m axis is 16%, so that the problems of anisotropy and high dislocation density exist in the nonpolar epitaxial material, and the quality of the epitaxial nonpolar GaN material has a larger difference from the practical application. The existing nonpolar GaN film has two main problems, namely rough surface appearance and higher dislocation density. This is a major factor limiting the performance parameters of nonpolar GaN-based devices, and the advantages of nonpolar GaN-based devices are not clearly manifested.
Many in-situ defect reduction techniques are applied to the growth of nonpolar GaN materials, such as substrate nitridation, optimization of various growth conditions, a two-step growth method, a SiN insertion layer technique and a patterned substrate technique, wherein the two-step growth method (controlling the growth conditions, growing a three-dimensional GaN layer in a first step to reduce dislocations, and then converting the growth into a two-dimensional GaN to improve the surface morphology) is a simple and effective method for reducing dislocations, but has problems, such as that in order to effectively reduce dislocations, the three-dimensional GaN layer needs to be grown as thick as possible, but the surface is very rough due to the excessively thick three-dimensional GaN layer, and the surface morphology cannot be completely improved due to the fact that the two-dimensional GaN layer is thick, so that the subsequent device growth is adversely affected.
Therefore, it is necessary to provide a method for obtaining a sapphire substrate with low dislocation density and good surface morphology, which can improve the quality of the non-polar GaN thin film, so as to solve the above problems. The invention adopts the epitaxial growth method for improving the quality of the nonpolar GaN material by inserting the InGaN/GaN superlattice structure, can improve the problems of the existing two-step growth method, and further improves the material quality.
The invention content is as follows:
the invention aims to overcome the defects in the prior art, and the quality of a nonpolar a-plane GaN thin film material growing on a sapphire substrate is improved, the dislocation density is reduced, and the surface appearance is improved by a Metal Organic Chemical Vapor Deposition (MOCVD) method. The growth steps are as follows:
the method comprises the following steps: putting the r-surface sapphire substrate on a substrate holder in an MOCVD reaction chamber, and baking at the temperature of 1000-1100 ℃ for 3-10 minutes
Step two: nitriding for 2-10 min in mixed atmosphere of nitrogen and ammonia in the volume ratio of 2 to 1 at 1000-1100 deg.c.
Step three: reducing the temperature to 500-600 ℃, and growing a low-temperature nucleating layer with the thickness of 20-40nm under the pressure of 500-600 mbar.
Step four: heating to 1000-1100 deg.C, pressure 300-.
Step five: growing a two-dimensional GaN layer with low pressure and low V/III ratio at the temperature of 1000-1100 ℃ and under the pressure of 50-200mbar and the V/III ratio of 50-300 for the first time, wherein the thickness of the two-dimensional GaN layer is 1-2 mu m.
Step six: lowering the temperature to 700-800 ℃ to grow an InGaN/GaN superlattice structure, wherein the In component of the InGaN layer is 5-20%. The thickness is 5-20nm, the thickness of the GaN layer is 5-10nm, firstly a GaN layer is grown, then an InGaN layer with the components and the thickness is grown, the GaN layer and the InGaN layer are alternately grown for 3-20 periods, and finally a GaN layer with the thickness of 5-20nm is grown;
step seven: heating to 1000-1100 deg.C, pressure 50-200mbar, V/III ratio 50-300, and growing two-dimensional GaN layer with low pressure and low V/III ratio in thickness of 2-5 μm.
The growth method is characterized in that the growth method is a metal organic chemical vapor deposition method, trimethyl gallium or triethyl gallium is used as a gallium source, trimethyl indium is used as an indium source, ammonia gas is used as a nitrogen source, and carrier gas is hydrogen gas and nitrogen gas.
The mechanism of the invention is characterized in that: by utilizing the MOCVD growth technology, the InGaN/GaN superlattice layer is inserted into the middle of the two-dimensional GaN layer through a two-step growth method (firstly growing the three-dimensional GaN layer and then growing the two-dimensional GaN layer on the basis) on the r-plane sapphire substrate and introducing the InGaN/GaN superlattice insertion layer. The conventional method is a two-step growth method, the three-dimensional nonpolar GaN film grows under the conditions of high pressure and high V/III ratio, but the surface appearance is rough, and the two-dimensional nonpolar GaN film grows under the conditions of low pressure and low V/III ratio on the basis of the rough surface appearance, so that the surface appearance can be improved, and the dislocation density can be reduced. However, the dislocation density of the nonpolar GaN thin film grown by the two-step growth method is still high, which is not favorable for the operation of semiconductor devices. Therefore, on the basis of a two-step growth method, the InGaN/GaN superlattice structure insertion layer is introduced into the middle of the two-dimensional GaN layer, the InGaN/GaN superlattice insertion layer has the capabilities of relieving stress generated due to different lattice constants and changing the dislocation transmission direction so as to cut off partial dislocation, and transmission of threading dislocation generated by mismatch of most of the sapphire substrate and the GaN epitaxial layer is blocked. Therefore, the grown nonpolar GaN film has lower dislocation density and better surface appearance. The dislocation can be further reduced and the quality of the nonpolar GaN material can be improved on the basis of the original two-step growth method.
Drawings
FIG. 1 is a schematic view showing a growth structure of the present invention in which an InGaN/GaN superlattice structure insertion layer is inserted between two-dimensional GaN layers
FIG. 2 shows a sample (11) without an InGaN layer interposed20) X-ray diffraction ω scan of a surface along the c-axis
FIG. 3 shows (11) of a sample (embodiment 1) in which an insertion layer of InGaN/GaN superlattice structure is inserted20) X-ray diffraction ω scan of a surface along the c-axis
FIG. 4 is an atomic force microscope surface topography of a sample without an inserted InGaN layer
FIG. 5 is an atomic force microscope surface morphology diagram of a sample (embodiment 1) inserted with an insertion layer of InGaN/GaN superlattice structure
Detailed Description
The invention is further described below with reference to embodiment 1 and the accompanying drawings:
the InGaN/GaN superlattice structure insertion layer is inserted on a r-plane sapphire substrate by a Metal Organic Chemical Vapor Deposition (MOCVD) method, so that the quality of a nonpolar a-plane GaN film is improved, the dislocation density is reduced, and the surface appearance is improved. As shown in fig. 1, the InGaN/GaN superlattice structure insertion layer is inserted between two-dimensional GaN layers, and the specific experimental steps are as follows:
the growth steps are as follows:
the method comprises the following steps: placing the r-surface sapphire substrate on a substrate holder in an MOCVD reaction chamber, and baking at 1050 ℃ for 3 minutes
Step two: nitriding is carried out for 10 minutes at 1050 ℃ in a mixed atmosphere of nitrogen and ammonia in a volume ratio of 2 to 1.
Step three: the temperature is reduced to 550 ℃, the pressure is 500mbar, and a low-temperature nucleation GaN layer with the thickness of 40nm is grown.
Step four: heating to 1050 deg.C, pressure 500mbar, V/III ratio 3000, growing high-pressure high V/III ratio three-dimensional GaN layer with thickness 2 μm.
Step five: a low-pressure, low-V/III-ratio two-dimensional GaN layer with a thickness of 2 μm is grown for the first time at 1050 ℃ and under a pressure of 50mbar and a V/III ratio of 100.
Step six: the temperature was lowered to 750 c and an InGaN/GaN superlattice structure insertion layer was grown In which the In composition of the InGaN layer was 10%. The thickness is 10nm, the thickness of the GaN layer is 5nm, a GaN layer is grown firstly, then an InGaN layer is grown, the GaN layer and the InGaN layer grow alternately for 20 periods, and finally a GaN layer with the thickness of 5nm is grown;
step seven: and heating to 1050 ℃, keeping the pressure at 50mbar and the V/III ratio at 100, and growing a low-pressure low-V/III-ratio two-dimensional GaN layer with the thickness of 5 mu m for the second time.
The growth method is a metal organic chemical vapor deposition method, trimethyl gallium is a gallium source, trimethyl indium is an indium source, ammonia gas is a nitrogen source, and carrier gas is hydrogen and nitrogen.
Test results, FIG. 2 shows the sample without InGaN layer inserted (11)20) Surface x-ray diffraction omega scan along c-axisFIG. 1 shows a half-width of 1148 arcsec; FIG. 3 shows (11) of a sample (embodiment 1) in which an insertion layer of InGaN/GaN superlattice structure is inserted20) An x-ray diffraction omega scanning graph along a c axis is formed on the surface, the half width is 1012arcsec, and 136arcsec is reduced compared with the half width of a sample without an inserted InGaN layer; indicating that inserting the InGaN/GaN superlattice structure improves the material quality.
FIG. 4 is an atomic force microscope surface topography of a sample without an inserted InGaN layer, with a root mean square roughness of 1.01 nm; FIG. 5 is an atomic force microscope surface topography of a sample (embodiment 1) inserted with an insertion layer of InGaN/GaN superlattice structure, the root mean square roughness of the surface being 0.88 nm; the sample of embodiment 1 after inserting the insertion layer of the InGaN/GaN superlattice structure reduces the roughness and has a flatter surface.
The nonpolar GaN film prepared in the embodiment 1 has low dislocation density and good surface appearance. The quality of the nonpolar GaN material is improved, and the defects of the prior art are improved.
Finally, it should be noted that: the above facts are the general embodiments of the present invention, not the limitations thereof; any simple changes or modifications in the technical solutions of the above embodiments, or any equivalent replacement of part or all of the technical solutions, should be included in the protection scope of the present invention.
Claims (1)
1. A method for improving the epitaxial quality of a nonpolar GaN material by inserting an InGaN/GaN superlattice structure is characterized in that the structure of an epitaxial wafer sequentially comprises the following steps from bottom to top: after a GaN nucleating layer grows on the r-surface sapphire substrate, a high-temperature three-dimensional GaN layer grows under the growth conditions of high pressure and high V/III ratio; a high-temperature two-dimensional GaN layer grown under the growth conditions of low pressure and low V/III ratio for the first time; an InGaN/GaN superlattice structure insertion layer; a high-temperature two-dimensional GaN layer grown under the growth conditions of low pressure and low V/III ratio for the second time;
the high-temperature three-dimensional GaN layer grown under the growth conditions of high pressure and high V/III ratio has the growth temperature of 1000-1100 ℃, the pressure of 300-600mbar, the V/III ratio, namely the molar flow ratio of the V-group source to the III-group source, of 1000-3000 and the thickness of 1-2 mu m;
the high-temperature two-dimensional GaN layer grown under the growth conditions of the first low pressure and the low V/III ratio has the growth temperature of 1000-1100 ℃, the pressure of 50-200mbar, the V/III ratio of 50-300 and the thickness of 1-2 mu m;
the InGaN/GaN superlattice structure insertion layer grows at the temperature of 700-800 ℃, wherein the mole percentage of an In component In the InGaN layer is 5% -20%, a GaN layer with the thickness of 5-20nm is grown firstly, then an InGaN layer with the thickness of 5-20nm of the In component is grown, the GaN layer and the InGaN layer alternately grow for 3-20 periods, and finally a GaN layer with the thickness of 5-20nm grows;
the high-temperature two-dimensional GaN layer grown under the growth conditions of the second low pressure and the low V/III ratio has the growth temperature of 1000-1100 ℃, the pressure of 50-200mbar, the V/III ratio of 50-300 and the thickness of 2-5 mu m.
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| CN105845798A (en) * | 2015-01-16 | 2016-08-10 | 北京大学 | Method of preparing warp-free group-III nitride composite substrate and substrate placing device |
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